WO2022059578A1 - 粉体、化粧料用白色顔料、化粧料 - Google Patents

粉体、化粧料用白色顔料、化粧料 Download PDF

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Publication number
WO2022059578A1
WO2022059578A1 PCT/JP2021/033013 JP2021033013W WO2022059578A1 WO 2022059578 A1 WO2022059578 A1 WO 2022059578A1 JP 2021033013 W JP2021033013 W JP 2021033013W WO 2022059578 A1 WO2022059578 A1 WO 2022059578A1
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Prior art keywords
powder
volume
thickness
diameter
crystal particles
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PCT/JP2021/033013
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English (en)
French (fr)
Japanese (ja)
Inventor
真弓 岩國
圭史 芦▲高▼
直也 三輪
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株式会社フジミインコーポレーテッド
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Priority to EP21869265.5A priority Critical patent/EP4215176A4/en
Priority to JP2022550502A priority patent/JPWO2022059578A1/ja
Priority to US18/245,761 priority patent/US20230390166A1/en
Priority to CN202180063119.1A priority patent/CN116490159A/zh
Priority to KR1020237008463A priority patent/KR20230069109A/ko
Publication of WO2022059578A1 publication Critical patent/WO2022059578A1/ja

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/0254Platelets; Flakes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216Solid or semisolid forms
    • A61K8/022Powders; Compacted Powders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • C01B25/372Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/42Colour properties
    • A61K2800/43Pigments; Dyes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/12Face or body powders for grooming, adorning or absorbing
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/54Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Definitions

  • the present invention relates to powders, white pigments for cosmetics, and cosmetics.
  • the white pigment for cosmetics is a base pigment for obtaining a cosmetic composition by mixing with other pigments.
  • titanium oxide (IV) TIM 2 , titanium dioxide; hereinafter, also simply referred to as “titanium oxide”
  • titanium dioxide has been generally used as a white pigment for cosmetics.
  • titanium dioxide has a high refractive index and excellent hiding power.
  • Patent Document 1 describes fan-shaped rutyl-type titanium oxide particles in which rod-shaped particles having a side size of 0.05 to 0.2 ⁇ m and a thickness direction of 0.02 to 0.1 ⁇ m are aggregated and / or bonded. Is further aggregated and formed, the particle size of the aggregated particles is 0.1 to 5.0 ⁇ m, and the average friction coefficient (MIU value) is 0.2 or more and less than 0.7. Aggregated particles are disclosed. According to the rutile-type titanium oxide agglomerated particles, when blended in cosmetics, especially make-up cosmetics, it can be applied smoothly to the skin, and there is no squeaky or rough feeling on the skin, and appropriate coloring is performed. It is stated that it is possible to produce the effect of producing a natural skin feeling without whitening due to the power and concealing power.
  • Patent Document 2 describes (A) 5 to 40% by weight of one or more solid waxes selected from microcrystalline wax, polyethylene polypropylene copolymer, polyethylene wax, selecin wax and paraffin wax, and (B) particle size. Contains 1 to 30% by weight of one or more fine particle powders selected from aluminum oxide of 0.1 ⁇ m or less and silicic anhydride, and (C) 30 to 80% by weight of liquid oil, incident angle, reflection angle. Described are oil-based solid cosmetics characterized by having a glossiness of 40% or more when both are 60 ° C.
  • Patent Document 3 describes at least one powder phase, one emulsifying system, one hydrophilic gelling agent, one organic lake, and at least one organopoly in a physiologically acceptable medium. Containing a siloxane elastomer and a hygroscopic hydrophilic active agent present in a content between 1% by weight and 40% by weight based on the total weight of the composition, based on the total weight of the composition.
  • a solid make-up and / or care cosmetic composition in the form of a compact powder with a solid content of 90% by weight or more has been described.
  • the composition contains 35% by mass or more of a powder phase (filler, pearl brightener, inorganic pigment, reflective particles) and contains 0.01% by mass to 20% by mass of the total amount of organic rake with respect to the total mass of the composition.
  • a powder phase contains 35% by mass or more of a powder phase (filler, pearl brightener, inorganic pigment, reflective particles) and contains 0.01% by mass to 20% by mass of the total amount of organic rake with respect to the total mass of the composition.
  • a powder phase contains 35% by mass or more of a powder phase (filler, pearl brightener, inorganic pigment, reflective particles) and contains 0.01% by mass to 20% by mass of the total amount of organic rake with respect to the total mass of the composition.
  • the hydrophilic gelling agent can be selected from thickening fillers, polymeric thickeners and associative polymers.
  • the composition of one particular embodiment preferably comprises a chelating agent selected from aminocarboxylic acids such as EDTA t
  • Patent Document 4 describes a cosmetic composition in the form of a water-in-oil solid emulsion in which an aqueous phase is dispersed in a lipid phase, wherein the lipid phase has a melting point of 25 to 42 ° C. and an average length of 0. It contains at least one type of wax in the form of a solid form of needle-like crystals with a shape coefficient of 1 to 50 ⁇ m and a shape coefficient of 2 or more, and the maximum force measured by texture during penetration of the probe into the composition is 0. Cosmetic compositions characterized by being .25 Newtons or higher are described.
  • the aqueous phase contains 50% by weight of water or an organic solvent miscible with water
  • the lipid phase contains 2 to 65% of liquid oil.
  • the composition may also contain a particle phase and is present in an amount of 0.01 to 40% by weight, more preferably 0.01 to 30% by weight, particularly 0.05 to 20% by weight, based on the total weight of the composition.
  • the cosmetic composition particularly contains a conventional pigment and / or a pearl component and / or a filler.
  • Pigment also means a white or colored, mineral or organic particle that is insoluble in a liquid hydrophilic phase and is used to impart color and / or opacity to the composition, filler.
  • Means colorless or white, mineral or synthetic, flaky or non-flaky particles, and the pearl component can mean particles of pearlescent or synthetic pearly luster produced from shell-bearing soft animals. Are listed.
  • Patent Document 5 contains (A) a powder composed of N ⁇ -monooctanoyl lysine, (B) an inorganic powder, and (C) an oil agent, and the content of the component (A) is the entire cosmetic composition.
  • the content of the component (B) is 0.1 to 95% by weight
  • the content of the component (B) is 4 to 99.5% by weight of the entire cosmetic composition
  • the content of the component (C) is 0.
  • the mixing ratio of the component (A) and the component (B) weight of the component (A): weight of the component (B)
  • the blending ratio of the component (C) (weight of the component (A): weight of the component (C)) is described as a cosmetic composition having a content of 15:85 to 75:25.
  • the inorganic powder examples include yellow iron oxide, red iron oxide, black iron oxide, fine iron oxide, bismuth oxychloride, carbon black, zinc oxide, etc., and the oil agent is usually used for cosmetics. If there is, it is not particularly limited, and it is described that, for example, vaseline, lanolin, celesin and the like can be mentioned.
  • titanium dioxide may be a carcinogen and will be classified in the carcinogenic category 2 under the CLP Regulation in the EU, so it is expected that its use in cosmetics will eventually be restricted.
  • An object of the present invention is to provide a powder having excellent hiding power that can be used in cosmetics as a white pigment instead of titanium dioxide.
  • one aspect of the present invention is a powder made of plate-shaped crystal particles, and the cumulative 50% primary particle diameter (volume D50% diameter) on a volume basis is 0.7 ⁇ m or more and 8.0 ⁇ m.
  • the white cosmetic pigment of this embodiment comprises titanium phosphate powder.
  • This titanium phosphate powder is composed of titanium phosphate crystal particles.
  • the titanium phosphate crystal particles are plate-like crystal particles.
  • the value obtained by measuring the thickness of the side surface of this plate-shaped crystal and calculating the cumulative 50% thickness (volume D50% thickness) based on the volume is 0.01 ⁇ m or more and less than 1.00 ⁇ m, and the aspect ratio (volume).
  • the value obtained by dividing the D50% diameter by the volume D50% thickness) is 5 or more.
  • the white pigment for cosmetics of this embodiment is composed of titanium phosphate powder composed of plate-like crystal particles of titanium phosphate, and the volume D50% diameter of the titanium phosphate powder is 0.7 ⁇ m or more and 8.0 ⁇ m or less.
  • the fluctuation coefficient (CV value) of the primary particle size of the titanium phosphate powder is 1.0 or less. Therefore, the cosmetic containing this is excellent in hiding power.
  • the volume D50% thickness of the plate-shaped crystal particles is less than 0.01 ⁇ m, the plate-shaped particles are not formed, and if it exceeds 1.00 ⁇ m, the hiding power is lowered, so that the thickness of the plate-shaped crystal particles ( Volume D50% thickness) shall be 0.01 ⁇ m or more and 1.00 ⁇ m or less.
  • the aspect ratio is 5 or more, the slipperiness is also excellent.
  • This titanium phosphate powder can be obtained, for example, by the following method. First, an aqueous solution of titanyl sulfate and an aqueous solution of phosphoric acid are mixed at a ratio of the molar concentration of phosphorus [P] to the molar concentration of titanium [Ti] [P] / [Ti] of 5 or more and 21 or less to prepare a mixed solution. obtain. Next, this mixed solution is placed in a closed container, the temperature is maintained at a value within the range of 100 ° C. or higher and 160 ° C. or lower, and the reaction is carried out for a predetermined time (for example, 5 hours or longer). That is, hydrothermal synthesis is performed.
  • a predetermined time for example, 5 hours or longer
  • the pressure inside the closed container is higher than the atmospheric pressure naturally determined by the pressurizing temperature. As a result, a slurry containing crystal particles of titanium phosphate is obtained. Next, after cooling the obtained slurry, solid content (titanium phosphate crystal particles) is separated from the slurry. The obtained solid content is washed with a washing solution consisting of water or aqueous ammonia (ammonium hydroxide), and then dried.
  • a washing solution consisting of water or aqueous ammonia (ammonium hydroxide
  • the white cosmetic pigment of this embodiment consists of boron nitride powder.
  • This boron nitride powder is composed of boron nitride crystal particles.
  • the boron nitride crystal particles are plate-like crystal particles.
  • the value obtained by measuring the thickness of the side surface of this plate-shaped crystal and calculating the cumulative 50% thickness (volume D50% thickness) based on the volume is 0.01 ⁇ m or more and less than 1.00 ⁇ m, and the aspect ratio (volume).
  • the value obtained by dividing the D50% diameter by the volume D50% thickness) is 5 or more.
  • the cosmetic containing the white pigment for cosmetics of this embodiment has excellent hiding power and excellent slipperiness as well as the cosmetic containing the white pigment for cosmetics of the first embodiment. It becomes.
  • the white pigment for cosmetics of this embodiment can be obtained by pulverizing a commercially available boron nitride powder.
  • Cosmetics consisting of a composition containing a powdery white pigment (hereinafter referred to as "cosmetic composition") include foundation, white powder, cheek red, eye color, manicure, make-up cosmetics such as lipstick, and whitening powder. , Body powder and other skin care cosmetics can be exemplified. Since the white pigments of the first and second embodiments have a large hiding power, they are suitable as white pigments for these cosmetic compositions.
  • the cosmetics those described in Patent Documents 2 to 5 are mentioned, and as the fine particle powder constituting the oil-based solid cosmetics of Patent Document 2, the solid make-up in the compact powder form of Patent Document 3 is used. And / or as an inorganic pigment of the powder phase constituting the care cosmetic composition, as a pigment of the particle phase constituting the cosmetic composition in the form of a water-in-oil solid emulsion of Patent Document 4, the cosmetic of Patent Document 5.
  • the inorganic powder constituting the composition the powder according to one aspect of the present invention can be used.
  • the powder of one aspect of the present invention can be treated with various polymers in order to improve cosmetic properties and pigment properties.
  • these treatment methods include fluorine treatment, silicon treatment, alkylsilane treatment, alkyl titanate treatment, metal soap treatment, lauroyl lysine treatment, ester treatment, and amino acid treatment.
  • amino acid treatment proline, hydroxyproline, alanine, glycine, sarcosine, aspartic acid, glutamic acid can be used.
  • a cosmetic containing a white pigment composed of the powder of one aspect of the present invention does not impair the effect of the present invention. Therefore, other components can be contained as needed.
  • Other ingredients include those commonly used in cosmetics, such as solvents, oils, surfactants, moisturizers, organic UV absorbers, antioxidants, thickeners, fragrances, colorants, bioactive ingredients, antibacterial agents. Examples include agents.
  • one kind may be used alone, or two or more kinds may be used in combination.
  • the content of other components is not particularly limited and can be appropriately set according to the purpose.
  • the content of the powder of one aspect of the present invention (for example, the titanium phosphate powder of the first embodiment and the boron nitride powder of the second embodiment) contained in the cosmetic is 0. It is preferably 1% by mass or more and 50% by mass or less.
  • the lid was opened to cool the slurry in the container to room temperature, and then the slurry was taken out from the container and filtered to separate the solid content from the slurry. After washing this solid content with water, it was dried (temperature 105 ° C., left for 24 hours) to obtain a powder.
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the obtained powder was observed with a scanning electron microscope, it was confirmed that the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter and CV value of the crystal particles constituting the obtained powder By analyzing the image of the scanning electron microscope using the image analysis software "Mac-View ver.4" manufactured by Mountech Co., Ltd., the volume D50% diameter and CV value of the crystal particles constituting the obtained powder When the volume D50% thickness was measured (standard deviation / number average primary particle diameter), the volume D50% diameter was 0.29 ⁇ m, the CV value was 0.45, and the volume D50% thickness was 0.030 ⁇ m. Met. Further, the aspect ratio of the crystal particles constituting the obtained powder was 10 by the calculation (0.29 / 0.030) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter, CV value (standard deviation / number average primary particle diameter), and volume D50% thickness of the crystal particles constituting the obtained powder were measured by the same method as that of the synthetic product A, the volume was measured.
  • the D50% diameter was 0.53 ⁇ m
  • the CV value was 0.34
  • the volume D50% thickness was 0.065 ⁇ m.
  • the aspect ratio of the crystal particles constituting the obtained powder was 8 by the calculation (0.53 / 0.065) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter, CV value (standard deviation / number average primary particle diameter), and volume D50% thickness of the crystal particles constituting the obtained powder were measured by the same method as that of the synthetic product A, the volume was measured.
  • the D50% diameter was 0.74 ⁇ m
  • the CV value was 0.42
  • the volume D50% thickness was 0.090 ⁇ m.
  • the aspect ratio of the crystal particles constituting the obtained powder was 8 by the calculation (0.74 / 0.090) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • ⁇ Synthetic product D> First, an aqueous solution of titanyl sulfate and an aqueous solution of phosphoric acid are mixed at a ratio of the molar concentration [P] of phosphorus [P] to the molar concentration [Ti] of titanium [P] / [Ti] to be 10.2 to obtain a mixed solution. rice field. Next, this mixed solution was placed in a 200 L autoclave, the temperature was maintained at 110 ° C., and the reaction was carried out for 5 hours. After the reaction, the lid was opened to cool the slurry in the container to room temperature, and then the slurry was taken out from the container and filtered to separate the solid content from the slurry. This solid content was washed with 29% aqueous ammonia (aqueous solution of ammonium salt) and then dried (temperature 105 ° C., left for 24 hours) to obtain a powder.
  • aqueous ammonia aqueous solution of ammonium salt
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter, CV value (standard deviation / number average primary particle diameter), and volume D50% thickness of the crystal particles constituting the obtained powder were measured by the same method as that of the synthetic product A, the volume was measured.
  • the D50% diameter was 1.11 ⁇ m
  • the CV value was 0.33
  • the volume D50% thickness was 0.143 ⁇ m.
  • the aspect ratio of the crystal particles constituting the obtained powder was 8 by the calculation (1.11 / 0.143) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • ⁇ Synthetic product E> First, an aqueous solution of titanyl sulfate and an aqueous solution of phosphoric acid are mixed at a ratio [P] / [Ti] of the molar concentration [P] of phosphorus to the molar concentration [Ti] of titanium to be 6.9 to obtain a mixed solution. rice field. Next, this mixed solution was placed in a 1.4 L autoclave, the temperature was maintained at 120 ° C., and the reaction was carried out for 5 hours. After the reaction, the lid was opened to cool the slurry in the container to room temperature, and then the slurry was taken out from the container and filtered to separate the solid content from the slurry. After washing this solid content with water, it was dried (temperature 105 ° C., left for 24 hours) to obtain a powder.
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter, CV value (standard deviation / number average primary particle diameter), and volume D50% thickness of the crystal particles constituting the obtained powder were measured by the same method as that of the synthetic product A, the volume was measured.
  • the D50% diameter was 2.07 ⁇ m
  • the CV value was 0.37
  • the volume D50% thickness was 0.302 ⁇ m.
  • the aspect ratio of the crystal particles constituting the obtained powder was 7 by the calculation (2.07 / 0.302) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • ⁇ Synthetic product F> First, an aqueous solution of titanyl sulfate and an aqueous solution of phosphoric acid are mixed at a ratio [P] / [Ti] of the molar concentration [P] of phosphorus to the molar concentration [Ti] of titanium to be 10.8 to obtain a mixed solution. rice field. Next, this mixed solution was placed in a 200 L autoclave, the temperature was maintained at 130 ° C., and the reaction was carried out for 5 hours. After the reaction, the lid was opened to cool the slurry in the container to room temperature, and then the slurry was taken out from the container and filtered to separate the solid content from the slurry. After washing this solid content with water, it was dried (temperature 105 ° C., left for 24 hours) to obtain a powder.
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter, CV value (standard deviation / number average primary particle diameter), and volume D50% thickness of the crystal particles constituting the obtained powder were measured by the same method as that of the synthetic product A, the volume was measured.
  • the D50% diameter was 7.44 ⁇ m
  • the CV value was 0.36
  • the volume D50% thickness was 0.856 ⁇ m.
  • the aspect ratio of the crystal particles constituting the obtained powder was 9 by the calculation (7.44 / 0.856) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • the synthesized titanium phosphate powders A to F were mixed at the ratios shown in Table 1 below to obtain titanium phosphate powders No. 1 to No. 9.
  • the titanium phosphate powders of Nos. 1 to 3 and No. 7 are the same as the titanium phosphate powders of the synthetic products A to D, respectively. Since the titanium phosphate powders of No. 4 to No. 6, No. 8 and No. 9 are mixed products, the volume D50% diameter, CV value and volume D50% thickness are measured by the above method. The aspect ratio was calculated. Further, a commercially available boron nitride powder (No.
  • No. 16 titanium phosphate powder was synthesized by the following method. First, an aqueous solution of titanyl sulfate and an aqueous solution of phosphoric acid are mixed at a ratio [P] / [Ti] of the molar concentration [P] of phosphorus to the molar concentration [Ti] of titanium to be 18.1 to obtain a mixed solution. rice field. Next, this mixed solution was placed in a 200 L autoclave, the temperature was maintained at 130 ° C., and the reaction was carried out for 10 hours. After the reaction, the lid was opened to cool the slurry in the container to room temperature, and then the slurry was taken out from the container and filtered to separate the solid content from the slurry. After washing this solid content with water, it was dried (temperature 105 ° C., left for 24 hours) to obtain a powder.
  • the particles constituting the powder were crystalline titanium phosphate having a structural formula of Ti (HPO 4 ) 2 ⁇ H 2 O. It could be confirmed.
  • the shape of the particles constituting the powder was plate-like and contained many hexagonal plate-like particles.
  • the volume D50% diameter, CV value (standard deviation / number average primary particle diameter), and volume D50% thickness of the crystal particles constituting the obtained powder were measured by the same method as that of the synthetic product A, the volume was measured.
  • the D50% diameter was 8.87 ⁇ m
  • the CV value was 0.38
  • the volume D50% thickness was 0.930 ⁇ m.
  • the aspect ratio of the crystal particles constituting the obtained powder was 10 by the calculation (8.87 / 0.930) using the measured values of the volume D50% thickness and the volume D50% diameter.
  • Table 2 shows the volume D50% diameter, CV value, volume D50% thickness, and aspect ratio of each powder.
  • the hiding power of each powder of No. 1 to No. 16 was measured by the following method. First, a slurry was obtained by adding 1.4 g of ethanol and 5.6 g of a 10% collodion solution to 3 g of each powder and mixing them. Next, the obtained slurry is applied and dried on a black-and-white concealment test paper with a film thickness of 100 ⁇ m in accordance with JIS K5600-4 (general paint test method-test method for visual characteristics of coating film). So, I got a test sample.
  • No. 3-5, No. 7-9, No. 12-14 titanium phosphate powder and boron nitride powder having a thickness of 0.01 ⁇ m or more and less than 1.00 ⁇ m have a high hiding power of 20 or more and 36 or less.
  • the hiding power of No. 7 titanium phosphate powder was higher than that of No. 15 titanium dioxide powder.
  • Titanium Phosphate Powder having a volume D50% diameter of less than 0.7 ⁇ m and No. 11 boron nitride powders, and No. 6 having a CV value of more than 1.0.
  • Titanium Phosphate Powder No. 16 Titanium Phosphate Powder with a volume D50% diameter of more than 8.0 ⁇ m, and No. 10 Boron Nitride Powder with a volume D50% diameter of more than 8.0 ⁇ m , 15, 14, 9, 7, 12, 18 respectively, which were low.
  • the titanium phosphate powder and boron nitride powder of Nos. 3 to 5, No. 7 to 9, and No. 12 to 14 have a hiding power that can be used in cosmetics as a white pigment in place of titanium dioxide. It was an excellent powder. Further, when the aspect ratio is 5 or more, the effect of excellent slipperiness can be obtained. Further, the titanium phosphate powder and the boron nitride powder of No. 5, No. 7, and No. 12 had a particularly high hiding power of 29 or more. That is, a powder composed of plate-shaped crystal particles having a volume-based cumulative 50% primary particle diameter (volume D50% diameter) of 0.97 ⁇ m or more and 1.84 ⁇ m or less is preferable because it has a particularly high hiding power.
  • titanium phosphate powder composed of plate-shaped crystal particles having a cumulative 50% thickness (volume D50% thickness) based on the volume of the plate-shaped crystal particles is 0.142 ⁇ m or more and 0.143 ⁇ m or less. , It is preferable because it has a particularly high hiding power.
  • the whiteness, refractive index, oil absorption amount, and specific surface area of each powder of No. 1 to No. 16 were measured by the following methods.
  • the whiteness was measured using an ultraviolet-visible spectrophotometer "UV-2450" manufactured by Shimadzu Corporation under the conditions of illumination D65 and a field of view of 2 °. That is, the whiteness of each powder was measured by a method according to JIS Z 8715.
  • each of the obtained powders and methyl polymethacrylate (membrane substrate: a transparent resin that is the base of the film) are put into N-methylpyrrolidone (a solvent that can dissolve the film substrate) and mixed. Then, the powder was dispersed to obtain a liquid in which polymethyl methacrylate was dissolved. A plurality of this liquid was obtained by changing the content of the powder. Using these liquids, a coating film having a thickness of 600 ⁇ m was formed on a PET film and dried at 80 ° C. to form a film consisting only of powder and resin. After cooling, the film was stripped from the PET film.
  • N-methylpyrrolidone a solvent that can dissolve the film substrate
  • the refractive indexes of the plurality of films thus obtained were measured using a refractometer "Prism Coupler Model 2010 / M" manufactured by Metallikon and a helium-neon laser light having a wavelength of 632.8 nm as a light source.
  • the measured values of the refractive indexes of the plurality of films were plotted on a graph with the horizontal axis as the powder content (volume%) and the vertical axis as the refractive index, and each plot was approximated by a straight line.
  • the value of the refractive index at the point where this straight line was extrapolated to the point where the content of the powder became 100% was defined as the refractive index of the powder.
  • the oil absorption was measured per 100 g by a method according to JIS K 5101-13.
  • the specific surface area was measured by the BET flow method using a fully automatic specific surface area measuring device "Macsorb (registered trademark) HM-1210" of Mountech Co., Ltd.
  • the ratio (oil absorption amount / specific surface area) of the oil absorption amount (ml / 100 g) to the specific surface area (m 2 / g) of the crystal particles in each powder was calculated.
  • SA in Table 3 indicates the specific surface area.
  • each powder of No. 1 to No. 9 and No. 16 has a high whiteness of 92.91 or more measured in accordance with JIS Z 8715, it can exhibit a high function as a base pigment.
  • each powder of No. 1 to No. 9 and No. 16 has a refractive index of 1.67 or more and less than 1.80, which is moderately higher than the refractive index of human skin (1.5).
  • a cosmetic composition containing a powder it is possible to obtain a natural finish that does not cause whitening with an appropriate covering power.
  • the cosmetic composition in which each powder is blended has less stickiness of the coating film and has a long-lasting makeup.

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PCT/JP2021/033013 2020-09-18 2021-09-08 粉体、化粧料用白色顔料、化粧料 WO2022059578A1 (ja)

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EP21869265.5A EP4215176A4 (en) 2020-09-18 2021-09-08 POWDER, WHITE PIGMENT FOR COSMETICS AND COSMETICS
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US18/245,761 US20230390166A1 (en) 2020-09-18 2021-09-08 Powder, white pigment for cosmetic, and cosmetic
CN202180063119.1A CN116490159A (zh) 2020-09-18 2021-09-08 粉体、化妆品用白色颜料、化妆品
KR1020237008463A KR20230069109A (ko) 2020-09-18 2021-09-08 분체, 화장료용 백색 안료, 화장료

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